头孢克肟中一种新的聚合物杂质及其结构分析

A New Polymer Impurity in Cefixime and Its Structure Analysis

摘要: 目的：对抗生素头孢克肟中的小分子杂质和聚合物杂质进行深入研究。方法：采用TSK凝胶色谱和反相液相色谱质谱联用和二维液相色谱质谱分析方法分析头孢克肟中的杂质成分，用制备液相方法制备出相应的杂质进行结构确认。结果：TSK凝胶色谱和反相液相色谱质谱联用及二维液相色谱质谱分析鉴定出头孢克肟中的一个新杂质(用imp表示)，且该小分子杂质能以二聚体聚合物杂质形式存在。将imp做了分离纯化制备和分析鉴定，结论：imp是在头孢克肟中新发现的杂质，在头孢克肟颗粒中其含量达0.13%，imp能以二聚体的形式存在。

Abstract: Objective: To study the small molecular impurities and polymer impurities in cefixime. Methods: the impurities in cefixime were analyzed by TSK-gel chromatography, RP-HPLC coupled with mass spectrometry and two-dimensional liquid chromatography-mass spectrometry. Results: a new im-purity imp in cefixime was identified by TSK-gel chromatography, reversed-phase liquid chroma-tography coupled with mass spectrometry and two-dimensional liquid chromatography-mass spec-trometry. The small molecule impurity can exist in the form of dimer polymer impurity. Imp was isolated, purified, prepared and identified. Conclusion: imp is a new impurity found in cefixime granules. The content of imp in cefixime granules is more than 0.1%, imp can exist in the form of dimer.